Uncovering interaction by QbD in optimization of stability-indicating HPLC method for simultaneous estimation of low-dose aspirin and lansoprazole

Abstract

In the present study a quality by design acquiescent method utilizing design of experiment and method operable design regions methodology was evaluated for optimization of chromatographic condition for separation of ten degradation products along with peaks of aspirin and lansoprazole. Box-Behnken design was exploited to evaluate the main and interaction effects of the selected critical process parameters on the critical quality attributes, viz resolution between the peak pairs and retention time of last eluting peak. The optimal separation was predicted at pH 3.6, with a gradient starting at 20% of acetonitrile and initial hold time of 10 min. The results of experimental methods show excellent agreement with predicted results, highlighting the importance of design of experiments in method optimization. The selected working condition was then fully validated according to International Conference on Harmonisation guidelines for linearity, range, accuracy, precision and robustness.